#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:53:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179216 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/43/4314319.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4314319
loop_
_publ_author_name
'Perumal Sekar'
'James A. Ibers'
_publ_section_title
;
 Synthesis and Characterization of HN(SPiPr2)(SePPh2) and
 [Te{N(SPiPr2)(SePPh2)}2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6294
_journal_page_last               6299
_journal_paper_doi               10.1021/ic030194u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C36 H48 N2 P4 S2 Se2 Te'
_chemical_formula_weight         982.28
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.9030(10)
_cell_angle_beta                 115.4710(10)
_cell_angle_gamma                92.281(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8476(9)
_cell_length_b                   10.3296(9)
_cell_length_c                   11.3429(10)
_cell_measurement_temperature    153(2)
_cell_volume                     1008.43(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11957
_diffrn_reflns_theta_full        28.82
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    2.833
_exptl_absorpt_correction_T_max  0.8892
_exptl_absorpt_correction_T_min  0.7547
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.669
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
  [1.00000+0.00000exp(0.00(sinθ/λ)²)]/
    [σ²(Fo²)+0.0000+0.0000*P+(0.0400P)²+0.0000sinθ/λ]
  where P = 1.00000Fo² + 0.00000Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                3761
_reflns_number_total             4751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030194u_2.cif
_cod_data_source_block           Te[N(SPiPr2)(SePPh2)]2
_cod_database_code               4314319
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Te Te 0.0000 0.5000 0.5000 0.02046(9) Uani 1 2 d S . .
Se1 Se -0.04033(3) 0.77124(3) 0.55853(3) 0.02343(10) Uani 1 1 d . . .
S1 S 0.22149(9) 0.56325(8) 0.43784(8) 0.02435(18) Uani 1 1 d . . .
P1 P 0.37147(9) 0.70417(8) 0.60615(8) 0.02047(18) Uani 1 1 d . . .
P2 P 0.18295(9) 0.82707(8) 0.73297(8) 0.01873(17) Uani 1 1 d . . .
N1 N 0.3189(3) 0.7602(2) 0.7190(3) 0.0207(5) Uani 1 1 d . . .
C1 C 0.4223(4) 0.8351(3) 0.5402(3) 0.0253(7) Uani 1 1 d . . .
H1A H 0.4991 0.9058 0.6179 0.030 Uiso 1 1 calc R . .
C2 C 0.4948(4) 0.7787(4) 0.4468(4) 0.0354(9) Uani 1 1 d . . .
H2A H 0.5213 0.8504 0.4124 0.053 Uiso 1 1 calc R . .
H2B H 0.4221 0.7074 0.3711 0.053 Uiso 1 1 calc R . .
H2C H 0.5868 0.7425 0.4978 0.053 Uiso 1 1 calc R . .
C3 C 0.2828(4) 0.8990(3) 0.4655(3) 0.0301(8) Uani 1 1 d . . .
H3A H 0.3120 0.9691 0.4308 0.045 Uiso 1 1 calc R . .
H3B H 0.2421 0.9383 0.5277 0.045 Uiso 1 1 calc R . .
H3C H 0.2049 0.8306 0.3904 0.045 Uiso 1 1 calc R . .
C4 C 0.5421(4) 0.6324(3) 0.6925(4) 0.0306(8) Uani 1 1 d . . .
H4A H 0.5702 0.5818 0.6230 0.037 Uiso 1 1 calc R . .
C5 C 0.6773(4) 0.7384(4) 0.7930(4) 0.0431(10) Uani 1 1 d . . .
H5A H 0.7658 0.6946 0.8365 0.065 Uiso 1 1 calc R . .
H5B H 0.6519 0.7903 0.8616 0.065 Uiso 1 1 calc R . .
H5C H 0.7009 0.7982 0.7455 0.065 Uiso 1 1 calc R . .
C6 C 0.5049(5) 0.5329(4) 0.7607(4) 0.0395(9) Uani 1 1 d . . .
H6A H 0.5957 0.4934 0.8077 0.059 Uiso 1 1 calc R . .
H6B H 0.4237 0.4622 0.6925 0.059 Uiso 1 1 calc R . .
H6C H 0.4713 0.5794 0.8258 0.059 Uiso 1 1 calc R . .
C7 C 0.2299(4) 1.0073(3) 0.7787(3) 0.0200(6) Uani 1 1 d . . .
C8 C 0.3831(4) 1.0633(3) 0.8448(3) 0.0278(7) Uani 1 1 d . . .
H8A H 0.4597 1.0069 0.8648 0.033 Uiso 1 1 calc R . .
C9 C 0.4239(4) 1.2015(3) 0.8814(4) 0.0361(9) Uani 1 1 d . . .
H9A H 0.5282 1.2392 0.9271 0.043 Uiso 1 1 calc R . .
C10 C 0.3129(4) 1.2839(3) 0.8513(3) 0.0322(8) Uani 1 1 d . . .
H10A H 0.3411 1.3782 0.8764 0.039 Uiso 1 1 calc R . .
C11 C 0.1615(4) 1.2299(3) 0.7852(3) 0.0292(7) Uani 1 1 d . . .
H11A H 0.0852 1.2866 0.7635 0.035 Uiso 1 1 calc R . .
C12 C 0.1212(4) 1.0923(3) 0.7504(3) 0.0230(7) Uani 1 1 d . . .
H12A H 0.0166 1.0555 0.7060 0.028 Uiso 1 1 calc R . .
C13 C 0.1688(3) 0.7840(3) 0.8746(3) 0.0221(7) Uani 1 1 d . . .
C14 C 0.1528(4) 0.8774(4) 0.9729(4) 0.0323(8) Uani 1 1 d . . .
H14A H 0.1516 0.9682 0.9683 0.039 Uiso 1 1 calc R . .
C15 C 0.1385(5) 0.8394(4) 1.0786(4) 0.0410(10) Uani 1 1 d . . .
H15A H 0.1281 0.9040 1.1460 0.049 Uiso 1 1 calc R . .
C16 C 0.1395(4) 0.7070(4) 1.0847(4) 0.0403(9) Uani 1 1 d . . .
H16A H 0.1307 0.6812 1.1571 0.048 Uiso 1 1 calc R . .
C17 C 0.1532(4) 0.6121(4) 0.9869(3) 0.0326(8) Uani 1 1 d . . .
H17A H 0.1514 0.5211 0.9908 0.039 Uiso 1 1 calc R . .
C18 C 0.1698(4) 0.6501(3) 0.8829(3) 0.0263(7) Uani 1 1 d . . .
H18A H 0.1818 0.5851 0.8167 0.032 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Te S1 180.0 . 2_566 ?
S1 Te Se1 91.231(19) . . ?
S1 Te Se1 88.769(19) 2_566 . ?
S1 Te Se1 88.769(19) . 2_566 ?
S1 Te Se1 91.231(19) 2_566 2_566 ?
Se1 Te Se1 180.0 . 2_566 ?
P2 Se1 Te 92.86(2) . . ?
P1 S1 Te 103.50(4) . . ?
N1 P1 C4 104.55(15) . . ?
N1 P1 C1 112.89(14) . . ?
C4 P1 C1 108.03(16) . . ?
N1 P1 S1 117.74(10) . . ?
C4 P1 S1 108.98(12) . . ?
C1 P1 S1 104.36(11) . . ?
N1 P2 C7 109.76(14) . . ?
N1 P2 C13 106.90(14) . . ?
C7 P2 C13 105.90(14) . . ?
N1 P2 Se1 117.08(10) . . ?
C7 P2 Se1 108.26(10) . . ?
C13 P2 Se1 108.39(10) . . ?
P2 N1 P1 139.40(17) . . ?
C3 C1 C2 110.8(3) . . ?
C3 C1 P1 110.5(2) . . ?
C2 C1 P1 110.7(2) . . ?
C6 C4 C5 111.5(3) . . ?
C6 C4 P1 108.5(2) . . ?
C5 C4 P1 112.8(2) . . ?
C12 C7 C8 118.4(3) . . ?
C12 C7 P2 123.1(2) . . ?
C8 C7 P2 118.5(2) . . ?
C9 C8 C7 120.2(3) . . ?
C10 C9 C8 120.1(3) . . ?
C11 C10 C9 120.2(3) . . ?
C10 C11 C12 119.5(3) . . ?
C7 C12 C11 121.5(3) . . ?
C14 C13 C18 118.8(3) . . ?
C14 C13 P2 122.4(3) . . ?
C18 C13 P2 118.7(2) . . ?
C13 C14 C15 120.6(3) . . ?
C16 C15 C14 119.6(3) . . ?
C17 C16 C15 120.7(3) . . ?
C16 C17 C18 119.8(3) . . ?
C17 C18 C13 120.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te S1 2.6609(8) . ?
Te S1 2.6609(8) 2_566 ?
Te Se1 2.8278(4) . ?
Te Se1 2.8278(4) 2_566 ?
Se1 P2 2.1837(9) . ?
S1 P1 2.0499(11) . ?
P1 N1 1.591(3) . ?
P1 C4 1.821(3) . ?
P1 C1 1.824(3) . ?
P2 N1 1.583(3) . ?
P2 C7 1.809(3) . ?
P2 C13 1.811(3) . ?
C1 C3 1.531(5) . ?
C1 C2 1.549(4) . ?
C4 C6 1.527(5) . ?
C4 C5 1.528(5) . ?
C7 C12 1.384(4) . ?
C7 C8 1.398(4) . ?
C8 C9 1.392(5) . ?
C9 C10 1.382(5) . ?
C10 C11 1.377(5) . ?
C11 C12 1.387(4) . ?
C13 C14 1.385(4) . ?
C13 C18 1.405(4) . ?
C14 C15 1.395(5) . ?
C15 C16 1.384(5) . ?
C16 C17 1.378(5) . ?
C17 C18 1.387(5) . ?
